EP0356138B1 - Stabilisation de revêtements de filaments essorés par soufflage - Google Patents

Stabilisation de revêtements de filaments essorés par soufflage Download PDF

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Publication number
EP0356138B1
EP0356138B1 EP89308342A EP89308342A EP0356138B1 EP 0356138 B1 EP0356138 B1 EP 0356138B1 EP 89308342 A EP89308342 A EP 89308342A EP 89308342 A EP89308342 A EP 89308342A EP 0356138 B1 EP0356138 B1 EP 0356138B1
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EP
European Patent Office
Prior art keywords
filament
gas
containment vessel
radicals
chloride
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP89308342A
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German (de)
English (en)
Other versions
EP0356138A1 (fr
Inventor
Malcolm Allan Robertson
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Australian Wire Industries Pty Ltd
Original Assignee
Australian Wire Industries Pty Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Australian Wire Industries Pty Ltd filed Critical Australian Wire Industries Pty Ltd
Priority to AT89308342T priority Critical patent/ATE96473T1/de
Publication of EP0356138A1 publication Critical patent/EP0356138A1/fr
Application granted granted Critical
Publication of EP0356138B1 publication Critical patent/EP0356138B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C23C2/261—After-treatment in a gas atmosphere, e.g. inert or reducing atmosphere
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C23C2/28—Thermal after-treatment, e.g. treatment in oil bath
    • C23C2/29—Cooling or quenching
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/34—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the shape of the material to be treated
    • C23C2/36—Elongated material
    • C23C2/38—Wires; Tubes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S118/00—Coating apparatus
    • Y10S118/19—Wire and cord immersion

Definitions

  • the present invention relates to a process for the stabilisation of a molten metallic coating on a metallic filament prior to cooling to produce a shiny lustre on the metal coating, and to means for bringing about this stabilisation.
  • the performance of the granular layer wiping method was improved by the injection of a reactive gas such as hydrogen sulphide into the granular layer in a process known as gas wiping and described more fully in Australian patent specification 421,751.
  • a reactive gas such as hydrogen sulphide
  • gas wiping a process known as gas wiping and described more fully in Australian patent specification 421,751.
  • the primary purpose of the reactive gas is to form a layer of metal sulphide on the metal bath and within the granular layer to assist in the physical wiping of the excess metal from the filament.
  • Solidification of the coating metal is normally achieved by passing the filament through a cooling fluid, normally water and/or air. It has been found, in the gas jet wiping process, that it can be difficult to cool the filament without causing the resultant coating to have a rough surface. It has also been found that the solidified coating has a dull appearance; both of these characteristics are undesirable.
  • the present invention is directed to a method for the coating of a metallic filament with a molten metal, generally of the type disclosed in JP-A-61183456, comprising the steps of drawing the filament from a molten metal bath, passing the filament through a gas jet wiping nozzle having a gas orifice spaced apart from the molten metal bath to direct a wiping gas stream against the filament to wipe excess molten metal from the filament, passing the wiped filament through a gas containment vessel containing a reactive gas atmosphere including radicals or materials which will decompose to produce such radicals, the containment vessel being spaced from the gas jet wiping nozzle sufficiently to allow the venting of wiping gas therebetween such that the reactive gas is not adversely diluted, and then cooling the filament by applying thereto a fluid coolant.
  • JP-A-61183456 is not to form a stabilizing coating on the surface of the wiped filament by reaction between a reactive gas atmosphere and the molten metal drawn from the molten metal bath.
  • the object of the prior process is to form aluminium in situ in a reaction chamber and for this aluminium to be adhered to, the zinc deposited on the filament during the hot dip galvanizing step.
  • This prior process used aluminium chloride and hydrogen gas, whereby hydrogen chloride is produced, for forming the aluminium coating.
  • the present invention is characterised in that (a) the radicals which are chloride or sulphide radicals, or materials which will decompose to produce such radicals, are present in the containment vessel in sufficient quantity, and (b) the gas containment vessel is sufficiently long in relation to the speed of passage of the filament through the containment vessel that the filament has a long enough residence time in the containment vessel, to allow the reactive gas to react with the molten metal on the filament to form a stabilizing coating of metal sulphide or chloride on the surface of the wiped filament.
  • the present invention enables filaments of acceptable surface quality to be produced over a wider range of conditions than has previously been possible with gas jet wiping. It has been found that, depending on the shape of the filament, the thickness of the coating metal and the flow rate of the cooling fluid, there is a speed of passage of the filament above which the degree of the filament's surface smoothness is unacceptable (which term is taken to mean that the roughness can be felt by scraping ones fingernail longitudinally along the filament) if the invention is not used. The flatter the filament is (i.e. the larger its radius of curvature), and consequently the greater the resistance offered to the flow of the cooling fluid, the slower the filament must be processed in order to achieve acceptable surface quality.
  • the filament is preferably ferrous wire or rod however the process is also applicable to filaments in the form of tubular products, strip products whether planar or shaped in cross-section, and sheet products.
  • the term "filament” used in the description and claims is to be construed as encompassing all such products.
  • the coating metal is preferably zinc however other coating metals such as zinc alloys containing a majority of zinc may also be used.
  • the jet wiping nozzles for use in the present invention may be any one of the conventional jet wiping nozzles known, for example, from the following patent specifications:- U.S. 2,194,565 3,060,889 3,270,364 3,459,587 3,533,761 3,611,986 3,707,400 3,736,174 Australian 458,892 537,944 539,396 544,277 It is preferred, however, to use the jet wiping nozzle the subject of the present applicant's copending Australian Patent Application No. PJ 0032 entitled "Improved Product and Process" and corresponding EP Appln. No. 89308343.6, Publication No. 0357297 filed on 17th August 1989.
  • This specification discloses a gas jet wiping nozzle for use in controlling the film applied from the dip coating of a metal filament through a liquid metal bath, the nozzle having:
  • the wiping gas may be an oxidising gas such as air or, preferably, a non-oxidising gas such as nitrogen.
  • the containment vessel should be spaced apart from the gas jet wiping nozzle sufficiently for that part of the wiping gas stream that flows in a direction away from the metal bath to be adequately vented between the nozzle and the containment vessel to such an extent that the reactive gas is not adversely diluted. If the two are too close together, the wiping effect of the gas jet nozzle may be deleteriously affected, and wiping gas entering the containment vessel through the aperture admitting wire into the vessel may adversely affect the formation of a stabilising film on the filament through dilution of the reactive gas. On the other hand some outward pressure from the wiping gas jet may prevent an undue flow of the reactive gas atmosphere out through the aperture which admits the filament into the vessel.
  • the cooling means may be any one of a number of known types wherein a stream of water or other liquid or a stream of a cooling gas is caused to contact the filament and its still molten coating.
  • the preferred cooling means is that described in Australian Patent Specification 462,301.
  • An air knife is preferably positioned between the reactive gas containment vessel and the cooling means to direct a stream of air across the wire. This air knife serves to prevent droplets of water from dropping into the molten metal bath or from running down the strand if for any reason it is necessary to stop the strand temporarily.
  • the reactive gas preferred is hydrogen sulfide however any gas that contains or provides the sulphide or chloride radical may be used.
  • any gas that contains or provides the sulphide or chloride radical may be used.
  • the reactive gas atmosphere is preferably comprised of reactive gas in a combustible carrier gas such as natural gas, liquified petroleum gas, or propane.
  • a combustible carrier gas such as natural gas, liquified petroleum gas, or propane.
  • the use of such a combustible carrier which can be burnt as it passes out from the gas containment vessel is particularly useful when the reactive gas is hydrogen sulphide or a mercaptan as the sulphide containing material can be combusted together with the combustible gas.
  • the reactive gas is preferably present in the reactive gas atmosphere in concentration by volume of greater than 0.01%, more preferably 0.5% to 1.5%.
  • the reactive gas containment vessel should be of sufficient length to allow reaction to take place between the reactive gas and the molten metal and to form a protective film on the molten wire. It has been found, for instance, that a containment vessel having a length of 15cm is satisfactory for the galvanising of a 2.5mm diameter steel wire at a speed of up to 1.5m/s at a coating mass of 300g/m2 and a hydrogen sulphide concentration of 0.5% by volume. If a larger diameter wire is to be treated or a faster speed or larger cooling mass is desired then a longer gas containment vessel is required.
  • a steel wire 10 is passed through a bath 11 containing molten zinc 12, around a skid 26, and emerges travelling substantially vertically upwardly.
  • the wire 10 passes through a jet wiping nozzle 16 which applies a wiping force to the wire 10 and strips excess molten zinc therefrom.
  • the wire then passes into a tubular gas containment vessel 17 having apertures at its upper and lower ends of sufficient size to allow the passage of the wire therethrough without the wire contacting the sides of the apertures.
  • a 1% concentration of hydrogen sulphide in natural gas is introduced into the lower end of the containment vessel 17 through an inlet 18.
  • the reactive gas stream emanates from the upper end 19 of the containment vessel 17 where it is burnt.
  • the hydrogen sulphide in the reactive gas mixture causes the formation of a protective zinc sulphide film on the surface of the molten zinc coating.
  • the wire 10 then passes through a series of cooling water streams passing from a water source 22 having water spouts 23 into a water drain 24.
  • the water streams issuing from spouts 23 cool the wire and its coating sufficiently to solidify the zinc such that its surface is not marred by its subsequent passage over rollers 25.
  • the wire 10 can be passed through the above apparatus at faster speeds and with thicker zinc coatings than with known means and still show a smooth shiny surface after being cooled. There is no evidence of surface blemish caused by impingement of the cooling water streams on the wire as is seen in the absence of the reactive gas treatment.
  • Table I shows the quality of the surface coating resulting from a variety of wire speeds and coating masses for 4.0mm steel wire galvanised by dip coating in a zinc bath and wiped through a gas jet wiping nozzle as described in Australian Patent specification PJ 0032 which has a filament orifice of 10mm, a gas orifice width of 0.70mm and was positioned 15mm above the surface of the zinc bath and cooled by direct contact by a water stream with a low water pressure. It can be seen that as the wire speed and the coating mass increase so the quality of the surface coating decreases.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Thermal Sciences (AREA)
  • Coating With Molten Metal (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Surgical Instruments (AREA)
  • Percussion Or Vibration Massage (AREA)
  • Detergent Compositions (AREA)
  • Removal Of Insulation Or Armoring From Wires Or Cables (AREA)
  • Surface Treatment Of Glass Fibres Or Filaments (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Manufacturing Of Electric Cables (AREA)
  • Heat Treatment Of Strip Materials And Filament Materials (AREA)

Claims (7)

  1. Procédé de revêtement d'un filament métallique (10) comprenant des fils, des tiges, des produits tubulaires, des produits en bande de section plane ou profilée et des produits en feuilles par un métal fondu (12) comprenant les étapes suivantes : passage du filament dans le bain de métal fondu (11), passage du filament dans une tuyère d'essorage par jet de gaz (16) ayant un orifice pour gaz écarté du bain de métal fondu (11), pour envoyer un courant de gaz d'essorage sur le filament (10) afin d'essorer le métal fondu en excès du filament, passage du filament essoré à travers un récipient contenant du gaz (17) qui contient une atmosphère de gaz réactif comprenant des radicaux ou des matériaux se décomposant en produisant ces radicaux, le récipient contenant le gaz (17) étant écarté de la tuyère d'essorage par jet de gaz (16) d'une manière suffisante pour permettre l'échappement du gaz d'essorage entre eux de façon que le gaz réactif ne soit pas dilué de manière défavorable, et refroidissement ultérieur du filament en y appliquant un fluide refroidisseur (22, 23), le procédé étant caractérisé en ce que (a) les radicaux, qui sont des radicaux chlorure ou sulfure ou des matériaux se décomposant en produisant ces radicaux, sont présents dans le récipient contenant le gaz en quantité suffisante et (b) que le récipient contenant le gaz (17) est suffisamment long par rapport à la vitesse de passage du filament à travers le récipient contenant le gaz pour que le filament ait un temps de séjour suffisamment long dans le récipient contenant le gaz pour que le gaz réactif puisse réagir avec le métal fondu sur le filament pour former un revêtement stabilisant de sulfure ou de chlorure métallique sur la surface du filament essoré.
  2. Procédé selon la revendication 1, dans lequel le filament est un fil de métal ferreux et le métal fondu est du zinc ou un alliage du zinc contenant principalement du zinc.
  3. Procédé selon la revendication 1 ou 2, dans lequel l'atmosphère de gaz réactif contient une source de radicaux sulfure ou chlorure, cette source étant choisie dans le groupe constitué du sulfure d'hydrogène, du chlore, du chlorure d'hydrogène, du chlorure d'ammonium, du disulfure de diéthyle, du disulfure de dipropyle, du disulfure de diméthyle, de l'éthylmercaptan, du propylmercaptan, du bisulfure de carbone et du méthylmercaptan.
  4. Procédé selon la revendication 1, 2 ou 3, dans lequel l'atmosphère de gaz réactif comprend une source de radicaux sulfure ou chlorure dans du gaz naturel, du gaz de pétrole liquéfié, du propane ou un autre gaz porteur combustible.
  5. Procédé selon l'une quelconque des revendications précédentes, dans lequel la source de radicaux sulfure ou chlorure est présente dans l'atmosphère de gaz réactif à une concentration de 0,5% à 1,5% en volume.
  6. Procédé selon l'une quelconque des revendications précédentes, dans lequel le filament est refroidi en y appliquant de l'eau ou un autre liquide refroidisseur.
  7. Procédé selon l'une quelconque des revendications précédentes, dans lequel le récipient contenant le gaz (17) a une longueur d'au moins 15 cm et, de préférence, de 30 cm.
EP89308342A 1988-08-24 1989-08-17 Stabilisation de revêtements de filaments essorés par soufflage Expired - Lifetime EP0356138B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT89308342T ATE96473T1 (de) 1988-08-24 1989-08-17 Stabilisierung von beschichtungen auf abgestreiften faeden.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AUPJ003088 1988-08-24
AU30/88 1988-08-24

Publications (2)

Publication Number Publication Date
EP0356138A1 EP0356138A1 (fr) 1990-02-28
EP0356138B1 true EP0356138B1 (fr) 1993-10-27

Family

ID=3773313

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Application Number Title Priority Date Filing Date
EP89308342A Expired - Lifetime EP0356138B1 (fr) 1988-08-24 1989-08-17 Stabilisation de revêtements de filaments essorés par soufflage

Country Status (18)

Country Link
US (1) US5017407A (fr)
EP (1) EP0356138B1 (fr)
JP (1) JP2836853B2 (fr)
KR (1) KR0148569B1 (fr)
CN (1) CN1021234C (fr)
AT (1) ATE96473T1 (fr)
AU (1) AU616989B2 (fr)
BR (1) BR8904235A (fr)
CA (1) CA1332681C (fr)
DE (1) DE68910228T2 (fr)
ES (2) ES2045452T3 (fr)
IN (1) IN175062B (fr)
MX (1) MX170328B (fr)
MY (1) MY104171A (fr)
NO (1) NO302303B1 (fr)
NZ (1) NZ230395A (fr)
PT (1) PT91518B (fr)
ZA (1) ZA896282B (fr)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
WO2008025086A1 (fr) * 2006-08-30 2008-03-06 Bluescope Steel Limited Bande d'acier à revêtement métallique

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US5782903A (en) * 1987-10-19 1998-07-21 Medtronic, Inc. Intravascular stent and method
US5484449A (en) * 1992-01-07 1996-01-16 Medtronic, Inc. Temporary support for a body lumen and method
US5401317A (en) * 1992-04-01 1995-03-28 Weirton Steel Corporation Coating control apparatus
US6786971B2 (en) 1997-06-19 2004-09-07 Dean Robert Gary Anderson Method and apparatus for digital printing
US6190454B1 (en) 1997-06-19 2001-02-20 Dean Robert Gary Anderson Printer cartridge
US5972111A (en) 1997-06-19 1999-10-26 Anderson; Dean Robert Gary Metering device for paint for digital printing
US5944893A (en) * 1997-06-19 1999-08-31 Anderson; Dean Robert Gary Metering device for paint for digital printing
JP5221732B2 (ja) * 2010-10-26 2013-06-26 日新製鋼株式会社 ガスワイピング装置
US20130224385A1 (en) * 2011-04-21 2013-08-29 Air Products And Chemicals, Inc. Method and Apparatus for Galvanizing an Elongated Object
CN102994931B (zh) * 2012-11-20 2016-01-06 江苏高博智融科技有限公司 一种钢丝热镀锌后的抹拭方法
CN103215533A (zh) * 2013-05-07 2013-07-24 无锡盛力达科技股份有限公司 热镀锌生产线自动抹锌装置

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008025086A1 (fr) * 2006-08-30 2008-03-06 Bluescope Steel Limited Bande d'acier à revêtement métallique
US10233518B2 (en) 2006-08-30 2019-03-19 Bluescope Steel Limited Metal-coated steel strip

Also Published As

Publication number Publication date
CN1021234C (zh) 1993-06-16
PT91518A (pt) 1990-03-08
NO893398D0 (no) 1989-08-23
CN1040628A (zh) 1990-03-21
ES2045452T3 (es) 1994-01-16
DE68910228T2 (de) 1994-05-11
IN175062B (fr) 1995-04-29
NO302303B1 (no) 1998-02-16
AU616989B2 (en) 1991-11-14
AU3940589A (en) 1990-03-01
ES2047119T3 (es) 1994-02-16
JP2836853B2 (ja) 1998-12-14
CA1332681C (fr) 1994-10-25
EP0356138A1 (fr) 1990-02-28
MY104171A (en) 1994-02-28
JPH02104652A (ja) 1990-04-17
ATE96473T1 (de) 1993-11-15
KR0148569B1 (ko) 1998-11-02
ZA896282B (en) 1990-05-30
DE68910228D1 (de) 1993-12-02
KR900003402A (ko) 1990-03-26
BR8904235A (pt) 1990-04-10
MX170328B (es) 1993-08-16
NO893398L (no) 1990-02-26
NZ230395A (en) 1991-03-26
PT91518B (pt) 1995-05-31
US5017407A (en) 1991-05-21

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